CN105669885B - A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing - Google Patents
A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
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Abstract
A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing, includes the following steps：（1）Control the shallower pentabromotoluene of low-temp reaction synthesis color；（2）To step（1）Obtained pentabromotoluene is purified；（3）Utilize step（2）Obtained pentabromotoluene synthesis pentabromobenzyl bromide；（4）By step（3）Obtained pentabromobenzyl bromide is purified；（5）Utilize step（4）Obtained pentabromobenzyl bromide acrylic acid synthesizing pentabromobenzyl ester；（6）By step（5）Obtained acrylic acid pentabromobenzyl ester is polymerize, and molecular weight of product is accurately controlled by using composite initiator substep addition in polymerization process.This invention ensures that coloration, and improve purity and stability.
Description
Technical field
The present invention relates to polypentabrombenzamide acrylate synthesis technical field, a kind of specially high-purity high stability poly- third
Olefin(e) acid pentabromobenzyl ester industrialized process for preparing.
Background technology
Currently, polypentabrombenzamide acrylate belongs toPolymerizationType bromine systemFire retardant, bromine content is up to 71.7%, except having
Outside excellent flame-retarded efficiency, also there is excellent thermo-chemical stability, good processing performance and electric property, the phase with resin
Capacitive is good, has substantially no effect on the physics and machining property of material, and can improve by the impact strength of fire proofing.Polypropylene
When sour pentabromobenzyl ester is used for flame-retardant PBT, does not change the fusion temperature, crystallization temperature and latent heat of material, do not change material yet
Crystallinity.This explanation, this fire retardant system are in the noncrystalline domain of PBT, therefore to what does not have by the tensile strength of fire proofing
It influences.Since the polyacrylic acid ester moiety in polypentabrombenzamide acrylate can be effectively facilitated polymeric substrate and fire retardant
Compatibility, while also promoting the compatibility between treated glass fibre and pentabromobenzyl, therefore with polyacrylic acid pentabromobenzyl
When the fire-retardant PBT containing glass fibre of ester, the fire retardant frosting phenomenon that material is occurred after high temperature ageing is significantly reduced, simultaneously
The tensile strength and impact strength of material are maintained, and the bromine content for making material fire-retardant rank reach UL94V-O grades is smaller than
6phr.In addition, the pentabromobenzyl in polypentabrombenzamide acrylate can be invested by fire-retardant high polymer with excellent uviolresistance
Can, this, which is other many bromide fire retardants, to compare.Compared with other high molecular weight bromide fire retardants, polyacrylic acid five
Bromobenzyl ester also has a superior place, such as it is higher than the flame retarding efficiency of Brominated Polystyrene, but unlike Brominated Epoxy polymer
So that fire proofing is become fragile and material impact strength is caused to be decreased obviously.
Polypentabrombenzamide acrylate synthesizes mainly using toluene, bromine (or bromine-containing compound), acrylic acid as raw material, one
React gradually obtained under fixed condition.Toluene and the obtained pentabromotoluene of bromine reaction first, pentabromotoluene and bromine (or brominated chemical combination
Object) pentabromobenzyl bromide is obtained by the reaction, pentabromobenzyl bromide, which is further reacted with acrylic acid, is made pentabromobenzyl acrylate monomer, finally
Pentabromobenzyl acrylate occurs polymerisation under initiator effect and generates polypentabrombenzamide acrylate.
But in the prior art, since intermediate reaction step is more in polypentabrombenzamide acrylate building-up process, to it
The purity and color for mainly often walking product that product quality has an impact, especially pentabromotoluene are synthesized using pyroreaction,
It is not perfect along with existing purifying technique, cause the pentabromobenzyl bromide color subsequently synthesized deeper so that the face of final products
Color is deeper, and purity is relatively low, also affects the stability of product entirety.
Invention content
Technical problem solved by the invention is to provide a kind of high-purity high stability polypentabrombenzamide acrylate work
Industry preparation method, to solve the problems in above-mentioned background technology.
Technical problem solved by the invention is realized using following technical scheme：
A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing, includes the following steps：
（1）Control the shallower pentabromotoluene of low-temp reaction synthesis color；
（2）To step（1）Obtained pentabromotoluene is purified；
（3）Utilize step（2）Obtained pentabromotoluene synthesis pentabromobenzyl bromide；
（4）By step（3）Obtained pentabromobenzyl bromide is purified；
（5）Utilize step（4）Obtained pentabromobenzyl bromide acrylic acid synthesizing pentabromobenzyl ester；
（6）By step（5）Obtained acrylic acid pentabromobenzyl ester is polymerize, by using combination in polymerization process
Initiator substep addition accurately controls molecular weight of product.
In the present invention, as a kind of perferred technical scheme, the step（1）It is specific as follows：Bromine is put into a kettle
Element, for controlling reaction temperature at -5-10 DEG C, the weight ratio for controlling toluene and bromine is 1：（19-25）, toluene control is in 6-10h
It is added dropwise to complete, then insulation reaction, after reaction, steams extra bromine, centrifuge, material is washed to neutrality, obtains pentabromo- first
Benzene.
In the present invention, as a kind of perferred technical scheme, the step（2）It is specific as follows：By pentabromotoluene and solvent
It is heated to 40-50 DEG C, stirs 2h, then 0-5 DEG C of low temperature crystallization, product centrifugation can obtain pure white pentabromotoluene purity and can reach
99.5%。
In the present invention, as a kind of further preferred technical solution, the step（2）It is middle to use dichloroethanes, dichloro
One kind in methane, chloroform and carbon tetrachloride making solvent, and pentabromotoluene and weight of solvent ratio are 1:1-3.
In the present invention, as a kind of perferred technical scheme, the step（3）It is specific as follows：By pentabromotoluene, bromine,
Solvent is put into reaction kettle successively, is warming up to 50-70 DEG C, and insulation reaction 4-8h under ultraviolet light, reaction terminates, material is washed
To neutrality, centrifugation.
In the present invention, as a kind of further preferred technical solution, the step（3）In, the solvent used is dichloro
One kind in methane, dichloroethanes, chloroform and carbon tetrachloride, and the weight ratio of pentabromotoluene, bromine, solvent is 1：0.5-1：2-
3。
In the present invention, as a kind of perferred technical scheme, the step（4）It is specific as follows：Pentabromobenzyl bromide is put into
It in solvent, is stirred at 30-40 DEG C and washes 2h, product centrifugation, obtained product is fine white powder pentabromobenzyl bromide, and purity is
99.5% or more.
In the present invention, as a kind of further preferred technical solution, the step（4）The middle solvent used is dichloromethane
The weight ratio of one kind in alkane, dichloroethanes, chloroform and carbon tetrachloride, pentabromobenzyl bromide and solvent is 1:（2-2.4）.
In the present invention, as a kind of perferred technical scheme, the step（5）It is specific as follows：Successively by solvent, inhibition
Agent, acrylic acid put into reaction kettle, then put into natrium carbonicum calcinatum in 1.5-2h, and control temperature is less than 40 DEG C, keeps the temperature 1h
Afterwards, reactor temperature rises to 45-70 DEG C, puts into pentabromobenzyl bromide, then rise to temperature of reaction kettle in 1 hour 70 ~
Insulation reaction 3h between 130 DEG C, after sampling is qualified, material washing, recrystallization.99.5% or more, color is products obtained therefrom purity
Fine white powder.
In the present invention, as a kind of perferred technical scheme, the step（5）In solvent using dichloroethanes, dichloro
One kind in methane, chloroform, ethylene glycol monomethyl ether, polymerization inhibitor is using hydroquinone, tert-butyl phenol, p-hydroxyanisole, 1,4-benzoquinone
In one kind.
In the present invention, as a kind of perferred technical scheme, the step（6）It is specific as follows：It is added in a kettle molten
Agent walks the acrylic acid pentabromobenzyl ester of synthesis in addition, then starts logical nitrogen, is warming up to 60 DEG C, and the first step is then added and draws
Agent is sent out, second step initiator is added after 1-3 hour in heat preservation, insulation reaction 1-3 hour at 70 DEG C, and third is then added and walks initiation
Agent, in 80 DEG C of insulation reactions 1-3 hours.Reaction terminates, and centrifugation filters；The first step initiator, second step initiator and
Three step initiators are all made of one or more of bpo, AIBN, azobisisoheptonitrile.
In the present invention, as a kind of further preferred technical solution, the step（6）Middle solvent is using ethyl alcohol, different pungent
One kind in alcohol, glycol dimethyl ether, ethylene glycol monomethyl ether, chlorobenzene.
As a result of above technical scheme, the invention has the advantages that：
Present invention employs specific techniques to prepare pentabromotoluene, pentabromobenzyl bromide and acrylic acid pentabromobenzyl ester, protects
The final purity of product has been demonstrate,proved, meanwhile, pentabromotoluene, pentabromobenzyl bromide are purified immediately, use specific purification
Step not only ensure that coloration, and improve purity, in the course of the polymerization process, essence be added by using composite initiator substep
Really control molecular weight of product, can be obtained molecular weight 30000 or so, high-purity, the polypentabrombenzamide acrylate of high stability.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing, includes the following steps：
（1）The shallower pentabromotoluene of low-temp reaction synthesis color is controlled, it is specific as follows：Bromine is put into a kettle, is controlled
For reaction temperature processed at -5 DEG C, the weight ratio for controlling toluene and bromine is 1：19, toluene control is added dropwise to complete in 6h, is then kept the temperature
Reaction, after reaction, steams extra bromine, centrifuges, and material is washed to neutrality, obtains pentabromotoluene；
（2）To step（1）Obtained pentabromotoluene is purified, specific as follows：Pentabromotoluene and solvent are heated to 40
DEG C, 2h is stirred, then 0 DEG C of low temperature crystallization, product centrifugation can obtain pure white pentabromotoluene purity and can reach 99.5%, wherein adopt
Solvent is made with dichloroethanes, pentabromotoluene and weight of solvent ratio are 1:1；
（3）Utilize step（2）Obtained pentabromotoluene synthesis pentabromobenzyl bromide, it is specific as follows：By pentabromotoluene, bromine,
Solvent is put into reaction kettle successively, is warming up to 50 DEG C, and insulation reaction 4h under ultraviolet light, reaction terminates, during material is washed till
Property, centrifugation, the solvent used is dichloroethanes, and the weight ratio of pentabromotoluene, bromine, solvent is 1：0.5：2；
（4）By step（3）Obtained pentabromobenzyl bromide is purified, specific as follows：Pentabromobenzyl bromide is put into solvent,
It is stirred at 30 DEG C and washes 2h, product centrifugation, obtained product is fine white powder pentabromobenzyl bromide, and purity is 99.5% or more, is used
Solvent be dichloromethane, the weight ratio of pentabromobenzyl bromide and solvent is 1:2；
（5）Utilize step（4）Obtained pentabromobenzyl bromide acrylic acid synthesizing pentabromobenzyl ester, it is specific as follows：It successively will be molten
Agent, polymerization inhibitor, acrylic acid put into reaction kettle, then put into natrium carbonicum calcinatum in 1.5h, and control temperature is less than 40 DEG C,
After keeping the temperature 1h, reactor temperature rises to 45 DEG C, puts into pentabromobenzyl bromide, temperature of reaction kettle is then risen to 70 in 1 hour
DEG C insulation reaction 3h, after sampling is qualified, material washing, recrystallization.For products obtained therefrom purity 99.5% or more, color is pure white
Powder, solvent use dichloroethanes, polymerization inhibitor to use hydroquinone；
（6）By step（5）Obtained acrylic acid pentabromobenzyl ester is polymerize, by using combination in polymerization process
Initiator substep addition accurately controls molecular weight of product, specific as follows：Solvent is added in a kettle, the third of synthesis is walked in addition
Then olefin(e) acid pentabromobenzyl ester starts logical nitrogen, is warming up to 60 DEG C, first step initiator is then added, and heat preservation adds after 1 hour
Entering second step initiator, then insulation reaction 1 hour at 70 DEG C is added third and walks initiator, in 80 DEG C of insulation reactions 1 hour,
Reaction terminates, and centrifugation filters；The first step initiator, second step initiator and third step initiator are all made of bpo, and solvent is adopted
Use chlorobenzene.
Embodiment 2
A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing, includes the following steps：
（1）The shallower pentabromotoluene of low-temp reaction synthesis color is controlled, it is specific as follows：Bromine is put into a kettle, is controlled
For reaction temperature processed at 10 DEG C, the weight ratio for controlling toluene and bromine is 1：25, toluene control is added dropwise to complete in 10h, is then protected
Temperature reaction, after reaction, steams extra bromine, centrifuges, and material is washed to neutrality, obtains pentabromotoluene；
（2）To step（1）Obtained pentabromotoluene is purified, specific as follows：Pentabromotoluene and solvent are heated to 50
DEG C, 2h is stirred, then 5 DEG C of low temperature crystallizations, product centrifugation can obtain pure white pentabromotoluene purity and can reach 99.5%, wherein adopt
Solvent is made with carbon tetrachloride, pentabromotoluene and weight of solvent ratio are 1:3；
（3）Utilize step（2）Obtained pentabromotoluene synthesis pentabromobenzyl bromide, it is specific as follows：By pentabromotoluene, bromine,
Solvent is put into reaction kettle successively, is warming up to 70 DEG C, and insulation reaction 8h under ultraviolet light, reaction terminates, during material is washed till
Property, centrifugation, the solvent used is chloroform, and the weight ratio of pentabromotoluene, bromine, solvent is 1： 1： 3；
（4）By step（3）Obtained pentabromobenzyl bromide is purified, specific as follows：Pentabromobenzyl bromide is put into solvent,
It is stirred at 40 DEG C and washes 2h, product centrifugation, obtained product is fine white powder pentabromobenzyl bromide, and purity is 99.5% or more, is used
Solvent be chloroform, the weight ratio of pentabromobenzyl bromide and solvent is 1:2.4；
（5）Utilize step（4）Obtained pentabromobenzyl bromide acrylic acid synthesizing pentabromobenzyl ester, it is specific as follows：It successively will be molten
Agent, polymerization inhibitor, acrylic acid put into reaction kettle, then put into natrium carbonicum calcinatum in 2h, and control temperature is less than 40 DEG C, protects
After warm 1h, reactor temperature rises to 70 DEG C, puts into pentabromobenzyl bromide, temperature of reaction kettle is then risen to 130 DEG C in 1 hour
Insulation reaction 3h, after sampling is qualified, material washing, recrystallization.For products obtained therefrom purity 99.5% or more, color is pure white toner
End, solvent use ethylene glycol monomethyl ether, and polymerization inhibitor is using tert-butyl phenol, p-hydroxyanisole；
（6）By step（5）Obtained acrylic acid pentabromobenzyl ester is polymerize, by using combination in polymerization process
Initiator substep addition accurately controls molecular weight of product, specific as follows：Solvent is added in a kettle, the third of synthesis is walked in addition
Then olefin(e) acid pentabromobenzyl ester starts logical nitrogen, is warming up to 60 DEG C, first step initiator is then added, and heat preservation adds after 3 hours
Enter second step initiator, then insulation reaction 3 hours at 70 DEG C was added third and walks initiator, in 80 DEG C of insulation reactions 3 hours.
Reaction terminates, and centrifugation filters；The first step initiator, second step initiator use bpo, third walk initiator using AIBN,
Azobisisoheptonitrile, solvent use chlorobenzene.
Embodiment 3
A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing, includes the following steps：
（1）The shallower pentabromotoluene of low-temp reaction synthesis color is controlled, it is specific as follows：Bromine is put into a kettle, is controlled
For reaction temperature processed at 5 DEG C, the weight ratio for controlling toluene and bromine is 1：21, toluene control is added dropwise to complete in 8h, is then kept the temperature
Reaction, after reaction, steams extra bromine, centrifuges, and material is washed to neutrality, obtains pentabromotoluene；
（2）To step（1）Obtained pentabromotoluene is purified, specific as follows：Pentabromotoluene and solvent are heated to 45
DEG C, 2h is stirred, then 3 DEG C of low temperature crystallizations, product centrifugation can obtain pure white pentabromotoluene purity and can reach 99.5%, wherein adopt
Solvent, pentabromotoluene and weight of solvent ratio are done with one or both of dichloroethanes, dichloromethane, chloroform and carbon tetrachloride
It is 1:2；
（3）Utilize step（2）Obtained pentabromotoluene synthesis pentabromobenzyl bromide, it is specific as follows：By pentabromotoluene, bromine,
Solvent is put into reaction kettle successively, is warming up to 60 DEG C, and insulation reaction 4-8h under ultraviolet light, reaction terminates, and material is washed till
Neutrality, centrifugation, the solvent used is carbon tetrachloride, and the weight ratio of pentabromotoluene, bromine, solvent is 1：0.7：2.5；
（4）By step（3）Obtained pentabromobenzyl bromide is purified, specific as follows：Pentabromobenzyl bromide is put into solvent,
It is stirred at 35 DEG C and washes 2h, product centrifugation, obtained product is fine white powder pentabromobenzyl bromide, and purity is 99.5% or more, is used
Solvent be chloroform, the weight ratio of pentabromobenzyl bromide and solvent is 1:2.2；
（5）Utilize step（4）Obtained pentabromobenzyl bromide acrylic acid synthesizing pentabromobenzyl ester, it is specific as follows：It successively will be molten
Agent, polymerization inhibitor, acrylic acid put into reaction kettle, then put into natrium carbonicum calcinatum in 1.8h, and control temperature is less than 40 DEG C,
After keeping the temperature 1h, reactor temperature rises to 60 DEG C, puts into pentabromobenzyl bromide, temperature of reaction kettle is then risen to 100 in 1 hour
DEG C insulation reaction 3h, after sampling is qualified, material washing, recrystallization.For products obtained therefrom purity 99.5% or more, color is pure white
Powder, solvent use ethylene glycol monomethyl ether, polymerization inhibitor to use 1,4-benzoquinone；
（6）By step（5）Obtained acrylic acid pentabromobenzyl ester is polymerize, by using combination in polymerization process
Initiator substep addition accurately controls molecular weight of product, specific as follows：Solvent is added in a kettle, the third of synthesis is walked in addition
Then olefin(e) acid pentabromobenzyl ester starts logical nitrogen, is warming up to 60 DEG C, first step initiator is then added, and heat preservation is added after 2 hours
Then second step initiator, insulation reaction 2 hours at 70 DEG C were added third and walk initiator, in 80 DEG C of insulation reactions 2 hours.Instead
It should terminate, centrifugation filters；The first step initiator, second step initiator and third step initiator are all made of two different heptan of azo
Nitrile, solvent use isooctanol.
The performance of embodiment 1-3 is as follows：
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (9)
1. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing, it is characterised in that：Including following
Step：
(1) the shallower pentabromotoluene of control low-temp reaction synthesis color；
(2) pentabromotoluene obtained to step (1) purifies；
(3) the pentabromotoluene synthesis pentabromobenzyl bromide that step (2) obtains is utilized；
(4) pentabromobenzyl bromide that step (3) obtains is purified；
(5) the pentabromobenzyl bromide acrylic acid synthesizing pentabromobenzyl ester for utilizing step (4) to obtain；
(6) the acrylic acid pentabromobenzyl ester that step (5) obtains is polymerize, is caused by using combination in polymerization process
Agent substep addition accurately controls molecular weight of product；
The step (1) is specific as follows：Bromine is put into a kettle, and controlling reaction temperature controls toluene and bromine at -5-10 DEG C
The weight ratio of element is 1：(19-25), toluene control are added dropwise to complete in 6-10h, and then insulation reaction steams after reaction
Extra bromine, centrifugation, material are washed to neutrality, obtain pentabromotoluene.
2. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing as described in claim 1,
It is characterized in that：The step (2) is specific as follows：Pentabromotoluene and solvent are heated to 40-50 DEG C, stir 2h, then 0-5 DEG C it is low
Temperature crystallization, product centrifugation, can obtain pure white pentabromotoluene purity and can reach 99.5%.
3. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing as claimed in claim 2,
It is characterized in that：Solvent, pentabromo- are done using one kind in dichloroethanes, dichloromethane, chloroform and carbon tetrachloride in the step (2)
Toluene and weight of solvent ratio are 1:1-3.
4. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing as described in claim 1,
It is characterized in that：The step (3) is specific as follows：Pentabromotoluene, bromine, solvent are put into reaction kettle successively, are warming up to 50-70
DEG C, insulation reaction 4-8h under ultraviolet light, reaction terminates, and material is washed till neutrality, centrifugation.
5. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing as claimed in claim 4,
It is characterized in that：In the step (3), the solvent used for one kind in dichloromethane, dichloroethanes, chloroform and carbon tetrachloride,
And the weight ratio of pentabromotoluene, bromine, solvent is 1：0.5-1：2-3.
6. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing as described in claim 1,
It is characterized in that：The step (4) is specific as follows：By pentabromobenzyl bromide put into solvent in, stirred at 30-40 DEG C and wash 2h, product from
The heart, obtained product are fine white powder pentabromobenzyl bromide, and purity is 99.5% or more.
7. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing as claimed in claim 6,
It is characterized in that：The solvent used in the step (4) is one kind in dichloromethane, dichloroethanes, chloroform and carbon tetrachloride, and five
The weight ratio of bromo benzyl bromo and solvent is 1:(2-2.4).
8. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing as described in claim 1,
It is characterized in that：The step (5) is specific as follows：Successively by solvent, polymerization inhibitor, acrylic acid, put into reaction kettle, then in 1.5-
Natrium carbonicum calcinatum is put into 2h, control temperature is less than 40 DEG C, and after keeping the temperature 1h, reactor temperature rises to 45-70 DEG C, input five
Then temperature of reaction kettle is risen to the insulation reaction 3h between 70~130 DEG C by bromo benzyl bromo in 1 hour, after sampling is qualified, object
Material washing, recrystallization, for products obtained therefrom purity 99.5% or more, color is fine white powder, wherein solvent uses two chloroethenes
One kind in alkane, dichloromethane, chloroform, ethylene glycol monomethyl ether, polymerization inhibitor using hydroquinone, tert-butyl phenol, p-hydroxyanisole,
One or more of 1,4-benzoquinone.
9. a kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing as described in claim 1,
It is characterized in that：The step (6) is specific as follows：Solvent is added in a kettle, the acrylic acid pentabromobenzyl of synthesis is walked in addition
Then ester starts logical nitrogen, is warming up to 60 DEG C, first step initiator is then added, and heat preservation is added second step after 1-3 hours and causes
Then agent, insulation reaction 1-3 hours at 70 DEG C are added third and walk initiator, in 80 DEG C of insulation reactions 1-3 hours, reaction terminated,
Centrifugation filters；The first step initiator, second step initiator and third step initiator are all made of bpo, AIBN, two different heptan of azo
One or more of nitrile, solvent is using one kind in ethyl alcohol, isooctanol, glycol dimethyl ether, ethylene glycol monomethyl ether, chlorobenzene.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610052388.9A CN105669885B (en) | 2016-01-26 | 2016-01-26 | A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing |
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| CN201610052388.9A CN105669885B (en) | 2016-01-26 | 2016-01-26 | A kind of high-purity high stability polypentabrombenzamide acrylate industrialized process for preparing |
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| CN105669885A CN105669885A (en) | 2016-06-15 |
| CN105669885B true CN105669885B (en) | 2018-09-28 |
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| CN107446073B (en) * | 2017-08-03 | 2019-09-06 | 山东日兴新材料股份有限公司 | A kind of synthetic method of polypentabrombenzamide acrylate |
| JP7144924B2 (en) | 2017-08-22 | 2022-09-30 | ポリプラスチックス株式会社 | Flame-retardant polybutylene terephthalate resin composition |
| JP7079578B2 (en) * | 2017-08-22 | 2022-06-02 | ポリプラスチックス株式会社 | Flame-retardant polybutylene terephthalate resin composition |
| US11326053B2 (en) | 2018-03-22 | 2022-05-10 | Polyplastics Co., Ltd. | Flame-retardant polybutylene terephthalate resin composition |
| CN113174000B (en) * | 2021-03-31 | 2022-07-26 | 潍坊鑫洋化工有限公司 | Preparation method of poly (pentabromobenzyl acrylate) with controllable molecular weight |
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| CN1036385A (en) * | 1988-04-06 | 1989-10-18 | 山东省化学研究所 | The manufacture method of pentabromotoluene |
| CN102167762A (en) * | 2011-02-25 | 2011-08-31 | 山东润科化工股份有限公司 | Method for producing poly(pentabromobenzyl acrylate) |
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| CN1036385A (en) * | 1988-04-06 | 1989-10-18 | 山东省化学研究所 | The manufacture method of pentabromotoluene |
| CN102167762A (en) * | 2011-02-25 | 2011-08-31 | 山东润科化工股份有限公司 | Method for producing poly(pentabromobenzyl acrylate) |
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